CN110452421B - Dielectric composite material based on core-shell structure filler - Google Patents
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Abstract
The invention belongs to the field of dielectric composite materials, and particularly relates to a dielectric composite material based on core-shell structured packing. The specific technical scheme is as follows: the dielectric composite material comprises a ceramic material and a polymer, wherein the ceramic material is of a core-shell structure, and the dielectric constant of the shell structure is smaller than that of the core structure in the core-shell structure. The invention breaks through the traditional research thought of surface coating of barium titanate, adopts paraelectric phase strontium titanate as a shell layer, and prepares BaTiO by a two-step hydrothermal method3‑SrTiO3The composite core-shell filler is compounded with the polymer matrix to prepare the dielectric composite material, so that the interface polarization and the residual polarization of the composite material are reduced, the breakdown-resistant electric field is increased, and the energy storage density and the efficiency of the dielectric composite material are greatly improved. The dielectric composite material provided by the invention can be widely applied to various capacitors.
Description
Technical Field
The invention belongs to the field of dielectric composite materials, and particularly relates to a dielectric composite material based on core-shell structured packing.
Background
In recent years, the development of electronic technology is changing day by day, and capacitors are widely used in high-power devices, such as laser guns, radars, rail guns, electric shock generators, and space stations, because of their ultra-high power density. However, compared with electrochemical energy storage devices such as fuel cells, lithium ion batteries, and super capacitors, the capacitor still has the disadvantage of low energy density, so that electronic components applied to the capacitor are large in size, heavy in weight, and expensive in price, and the application and development of the capacitor are limited. Therefore, it is an effort of researchers to increase the energy density of the capacitor and to miniaturize the device.
Dielectric materials are important components of capacitors in terms of their energy density (U)e) The calculation formula of (2):
Ue＝∫EdD＝∫ε0εrEdE。
wherein E, ε0，εrThe breakdown field resistance, the vacuum dielectric constant and the relative dielectric constant of the material, respectively. It is known that to increase the energy density of a capacitor, it is necessary to increase the relative permittivity and the breakdown field resistance of a dielectric material.
At present, a great deal of research in the field is focused on an inorganic ceramic filler/polymer composite material system, and aims to combine the advantages of high dielectric constant of the inorganic filler with the advantages of high breakdown-resistant electric field and low dielectric loss of a polymer matrix, so that the dielectric composite material can obtain high dielectric constant and breakdown-resistant electric field at the same time, and further improve the energy storage density of the dielectric composite material.
Barium titanate, which is representative of conventional ferroelectric ceramics, has an ultra-high dielectric constant due to its spontaneous polarization characteristics, and thus is a popular choice for fillers in dielectric composites. Researchers have conducted a series of studies on the influence of barium titanate filler on the dielectric and energy storage properties of composite materials, for example, BaTiO was studied by Zhai David university3The nanospheres and the nanowires are used as fillers, and influence rules on the energy storage density of the PVDF-based dielectric composite material. Research shows that BaTiO3The ceramic filler can obviously improve the dielectric constant and the energy storage density of the composite material; with BaTiO3The increase of the filler content gradually increases the dielectric constant of the composite material.
But due to BaTiO3The ferroelectric ceramic has large dielectric loss, and the dielectric loss is increased along with BaTiO in the composite material3The increase of the content of the ceramic filler can not only gradually increase the residual polarization value of the composite material and increase the energy loss, but also introduce defects such as holes, cracks and the like into the composite material, so that the breakdown-resistant electric field value of the composite material is obviously reduced, and the storage of the composite material is limitedThe energy density is improved.
To address this problem, researchers have focused on BaTiO from the standpoint of interface engineering3The surface is coated with other shell ceramics with low dielectric constant to form a single-stage or multi-stage gradient interface, and the difference of the dielectric constant between the filler and the polymer is reduced to reduce the loss, thereby improving the energy storage density and the efficiency of the composite material.
For example, Lin et al, by coating on BaTiO3The surface of the nano-fiber is coated with a layer of non-ferroelectric ceramic TiO2Shell layer of TiO2The shell layer has low dielectric constant and non-ferroelectric property, so that the dielectric loss and the nonuniform electric field distribution of the composite material are reduced, and the energy storage density of the composite material is improved. Pan et al electrostatic spinning on BaTiO3Introducing Al to the surface of the nanofiber2O3And the insulating ceramic layer is used for reducing energy loss, improving the breakdown-resistant electric field of the composite material and obtaining high energy storage density and efficiency.
BaTiO that has been studied at present3-SiO2，BaTiO3-Al2O3Isonuclear shell filler systems of the type using BaTiO3The low-dielectric-constant shell layer is introduced into the low-dielectric-constant ceramic shell system prepared for the core, so that the mismatch of the dielectric constant between the filler and the polymer matrix and the local electric field concentration of the composite material are improved, the interface polarization is reduced, the breakdown-resistant electric field is further improved, and the energy storage density of the composite material is improved. But at the same time, the shell ceramics with low dielectric constant and BaTiO are introduced3The core has great crystal structure difference, and the interface of the core and the shell has the defects of cracks, holes and the like, which can be used as an additional transmission channel of charge carriers, and additional interface polarization is introduced into the dielectric composite material.
Therefore, it remains a difficult point in the art to provide a dielectric composite material with high energy storage density and high energy storage efficiency by increasing the breakdown field resistance while maintaining low remanent polarization.
Disclosure of Invention
The invention aims to provide a dielectric composite material with high energy storage density and energy storage efficiency.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows: the dielectric composite material comprises a ceramic material and a polymer, wherein the ceramic material is of a core-shell structure, the dielectric constant of the shell structure is smaller than that of the core structure in the core-shell structure, and the materials of the shell structure and the core structure are both perovskite structures.
Preferably, in the core-shell structure, the core structure material is BaTiO3(ii) a The shell structure material is SrTiO3。
Preferably, the preparation method of the core-shell structure comprises the following steps:
(1) a general reaction of Ba (OH)2·8H2Adding O into the acetic acid solution, and fully stirring and dissolving to obtain a solution 1;
(2) mixing TiCl4Adding the mixture into an ethanol solution to obtain a solution 2;
(3) uniformly mixing the solution 1 and the solution 2 to obtain a precursor solution;
(4) adding solid NaOH into the precursor solution, and fully and uniformly mixing to obtain an intermediate suspension;
(5) sr (OH)2·8H2Dissolving O in an acetic acid solution to obtain a solution 3;
(6) and adding the solution 3 into the intermediate suspension, fully and uniformly mixing, washing and drying a reaction product after hydrothermal reaction, and thus obtaining the required core-shell structure.
Preferably, the volume of the core-shell structure is 1 to 3 percent of the volume of the polymer.
Preferably, the preparation method of the dielectric composite material comprises the following steps:
(1) adding the core-shell material into an organic solvent, performing ultrasonic dispersion and fully stirring until the core-shell material is uniform;
(2) adding the polymer into a solvent, and fully dispersing to obtain a dielectric composite material solution;
(3) and carrying out tape casting on the dielectric composite material solution to obtain the dielectric composite material.
Accordingly, the dielectric composite material is used in a capacitor.
The invention has the following beneficial effects:
existing pair of BaTiO3The method for treating the filler is to directly coat a layer of material with low dielectric constant on the surface, and although the method can reduce dielectric loss and improve breakdown-resistant electric field, the method is easy to introduce defects at the interface of the core shell. The method breaks through the traditional method and leads SrTiO to be processed by a two-step hydrothermal method3Epitaxially grown on BaTiO3Surface preparation of BaTiO3-SrTiO3The core-shell filler is then compounded with a polymer matrix to prepare a dielectric composite material for energy storage application of a dielectric capacitor.
Wherein, the strontium titanate and the barium titanate used in the invention have the same perovskite structure and similar lattice constants. Strontium titanate with the same crystal structure as barium titanate is used as a shell layer, and the shell layer can be grown along the surface of the barium titanate by the strontium titanate in the hydrothermal reaction process to form an interface region with few defects, so that the dielectric constant mismatch between the filler and the matrix can be improved, the interface polarization can be reduced, and the generation of additional polarization can be reduced. More importantly, the strontium titanate is paraelectric phase at room temperature, has low remanent polarization value and dielectric loss, and is more beneficial to improving the energy storage efficiency of the composite material compared with the common low-dielectric constant material.
The dielectric composite material prepared by the method provided by the invention can effectively reduce the interface polarization and the residual polarization of the composite material, increase the breakdown-resistant electric field and further improve the energy storage density and the efficiency of the dielectric composite material.
Drawings
FIG. 1 shows BaTiO3-SrTiO3Scanning Electron Microscope (SEM) images of core-shell fillers;
FIG. 2 shows BaTiO3-SrTiO3Transmission Electron Microscopy (TEM) images of core-shell fillers;
FIG. 3 shows BaTiO3-SrTiO3High Resolution Transmission Electron Microscopy (HRTEM) images of core-shell fillers;
FIG. 4 shows BaTiO3-SrTiO3X-ray photoelectron spectroscopy (XPS) images of core-shell fillers;
FIG. 5 is a schematic diagram of P-E loop of the experimental group 1 and the control group 1 according to the present invention;
FIG. 6 is a comparison graph of breakdown-resistant electric fields, discharge energy densities and energy storage efficiencies of the experimental groups 1 to 3 and the control group 2 of the present invention.
Detailed Description
The invention comprehensively considers the structure and performance characteristics of strontium titanate, converts the conventional research idea of coating the surface of the ceramic filler, and leads SrTiO to be subjected to the two-step hydrothermal method3Epitaxially grown on BaTiO3Surface preparation of BaTiO3-SrTiO3Core-shell filler, and compounding the core-shell filler with a polymer matrix to obtain the novel dielectric composite material. Under the condition of lower content of core-shell filler, the dielectric composite material obtains better than a pure polymer matrix and BaTiO alone3Energy storage density of a dielectric composite that is a filler.
The preparation method is described in detail below with reference to specific examples.
The first embodiment is as follows: preparation of BaTiO3-SrTiO3Core-shell filler
The BaTiO3-SrTiO3The core-shell filler is prepared by a two-step hydrothermal method. 2.1809g of Ba (OH)2·8H2O was added to 16mL of a 1M acetic acid solution, and dissolved by stirring sufficiently to obtain a solution 1. Then 0.8mL of TiCl4To 16mL of absolute ethanol solution, solution 2 was obtained.
And uniformly mixing the solution 1 and the solution 2 to obtain a precursor solution. Then adding 5.0g of flaky NaOH into the precursor solution, and mechanically stirring for 10min to obtain the solution containing BaTiO3An intermediate suspension of nanoparticles and unreacted gel.
0.0967g Sr (OH)2·8H2O was dissolved in 24mL of 1M acetic acid solution to give solution 3. Said Ba (OH)2·8H2O、TiCl4And Sr (OH)2·8H2The amount of O is such that the molar ratio of Ba (Sr) to Ti is 1: 1.
Adding the solution 3 into the intermediate suspension, stirring and mixing uniformly, transferring the mixed suspension into a reaction kettle, carrying out hydrothermal reaction at 200 ℃ for 24 hours, and obtaining the reaction productWashing the product with anhydrous ethanol twice, and drying at 80 deg.C for 2 hr to obtain the desired BaTiO3-SrTiO3And (4) core-shell filler.
For the prepared BaTiO3-SrTiO3Scanning the core-shell filler by an electron microscope and a lens, wherein the result is shown in figures 1-3; and to BaTiO3-SrTiO3The core-shell filler was subjected to X-ray photoelectron spectroscopy, and the results are shown in FIG. 4.
Example two: preparation of dielectric composite materials
1. Three groups of BaTiO prepared in example one, 1 vol%, 2 vol% and 3 vol% of P (VDF-HFP) were weighed out using N, N-Dimethylformamide (DMF) as a solvent and a commercially available polyvinylidene fluoride-hexafluoropropylene copolymer (hereinafter abbreviated as P (VDF-HFP)) as a polymer, respectively3-SrTiO3Core-shell fillers as experimental groups 1, 2, 3; and respectively adding the mixture into a DMF solvent, ultrasonically dispersing for 30min, and stirring for 2h to fully and uniformly disperse.
Then adding solid P (VDF-HFP) with required mass into each group of solvents respectively, stirring for 12h at 50 ℃, and performing ultrasonic treatment for 1h to obtain BaTiO with good dispersibility3-SrTiO3Core shell filler/P (VDF-HFP) solution.
It will be appreciated that BaTiO is obtained as described above3-SrTiO3The core-shell filler/P (VDF-HFP) solution can be further dried according to actual needs by those skilled in the art to obtain the desired dielectric composite material, and further applied, for example, in the preparation of capacitor, etc. In the present embodiment, the solution is cast for convenience of subsequent data measurement, but the method is not limited to drying and molding. The specific method of the tape casting method is as follows:
the solution was dropped on a clean glass plate, and cast to prepare BaTiO using a fixed height applicator (SZQ)3-SrTiO3Drying the/P (VDF-HFP) composite material at 60 ℃ for 24h, hot-pressing at 200 ℃ for 20min, quenching in an ice-water mixture, and drying to obtain the required dielectric composite materials.
Simultaneously, under the same conditions, BaTiO3-SrTiO3Core-shell fillerBaTiO substituted with Polymer 1 vol%3Preparing a control group 1; pure P (VDF-HFP) polymer was used as control 2.
2. Respectively carrying out gold electrode sputtering on two surfaces of the dielectric composite materials of the experimental groups 1, 2 and 3 and the comparison groups 1 and 2 by utilizing magnetron sputtering equipment under the same condition; the sputtering power is 120W, and the sputtering time is 100 s.
Breakdown tests were performed on the dielectric composites of each experimental group: the voltage is increased continuously at the speed of 10kV/mm from 100V until the sample is broken down; the samples were tested for P-E loop (polarization-electric field curve) using a ferroelectric analyzer. The results are shown in FIGS. 5 and 6.
FIG. 5 is a P-E loop diagram of the dielectric composite of the experimental group 1 and the control group 1. As can be seen from FIG. 5, the residual polarization of the control group 1 was greater than that of the experimental group 1 at the same filler content, indicating that SrTiO3The introduction of the shell layer can effectively reduce the residual polarization value of the dielectric composite material. And calculating the discharge energy density of the composite material by integrating the tested P-E loop. It was calculated that the composite material of experimental group 1 obtained 13.89J/cm under its breakdown field resistance3Under the same conditions, the discharge energy density of control 1 under its breakdown-resistant electric field was 9.96J/cm3. It can be obtained that BaTiO is used3-SrTiO3The core-shell structure material is used as a filler, so that the interface polarization and the residual polarization of the dielectric composite material can be effectively reduced, a high breakdown-resistant electric field is obtained, and high discharge energy density and efficiency are further obtained.
Fig. 6 is a comparative graph of breakdown-resistant electric field, discharge energy density and energy storage efficiency of the control group 2 and the experimental groups 1, 2 and 3. The uppermost curve in fig. 6 is a variation curve of the breakdown field, and it can be seen that the dielectric composite materials of experimental groups 1, 2 and 3 can obtain the breakdown field higher than that of the comparative group 2 (pure P (VDF-HFP) polymer) at a low core-shell structure filler content (1 vol%, 2 vol% and 3 vol%). The middle curve of fig. 6 is a variation curve of the discharge energy density, and it can be seen that the discharge energy densities of the experimental groups 1, 2, and 3 are all higher than that of the control group 2. The lowest curve in fig. 6 is a variation curve of energy storage efficiency, and when the content of the core-shell filler is 1 vol% (experimental group 1), the energy storage efficiency is similar to that of pure P (VDF-HFP), and simultaneously, high discharge energy density is obtained.
Claims (5)
1. A dielectric composite characterized by: the dielectric composite material comprises a ceramic material and a polymer, wherein the ceramic material is in a core-shell structure, the dielectric constant of the shell structure is smaller than that of the core structure in the core-shell structure, and the material of the shell structure and the material of the core structure are both in perovskite structures; in the core-shell structure, the core structure material is BaTiO3The shell structure material is SrTiO3Said SrTiO3Epitaxially grown on BaTiO3A surface.
2. A dielectric composite material according to claim 1, wherein: the preparation method of the ceramic material comprises the following steps:
(1) a general reaction of Ba (OH)2·8H2Adding O into the acetic acid solution, and fully stirring and dissolving to obtain a solution 1;
(2) mixing TiCl4Adding the mixture into an ethanol solution to obtain a solution 2;
(3) uniformly mixing the solution 1 and the solution 2 to obtain a precursor solution;
(4) adding solid NaOH into the precursor solution, and fully and uniformly mixing to obtain an intermediate suspension;
(5) sr (OH)2·8H2Dissolving O in an acetic acid solution to obtain a solution 3;
(6) and adding the solution 3 into the intermediate suspension, fully and uniformly mixing, washing and drying a reaction product after hydrothermal reaction, and thus obtaining the required ceramic material.
3. A dielectric composite material according to claim 1, wherein: the volume of the ceramic material is 1-3% of the volume of the polymer.
4. A dielectric composite material according to claim 1, wherein: the preparation method of the dielectric composite material comprises the following steps:
(1) adding the ceramic material into an organic solvent, performing ultrasonic dispersion and fully stirring the mixture until the mixture is uniform;
(2) adding the polymer into a solvent, and fully dispersing to obtain a dielectric composite material solution;
(3) and carrying out tape casting on the dielectric composite material solution to obtain the dielectric composite material.
5. Use of the dielectric composite material as claimed in any one of claims 1 to 4 in a capacitor.
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